在线中空纤维膜液相微萃取/高效液相色谱法测定3种痕量芳香胺

Automated Determination of Three Kinds of Aromatic Amines by On-line Hollow Fiber Liquid-phase Microextraction / High Performance Liquid Chromatography

建立了一种在线中空纤维膜液相微萃取/高效液相色谱联用技术测定3种痕量芳香胺（邻甲苯胺、3,3＇-二甲基联苯胺、2-萘胺）的新方法,以顺序注射仪将中空纤维膜液相微萃取装置和高效液相色谱仪连接搭建在线检测装置,利用此装置优化了萃取溶剂、供体相、接收相、盐效应、搅拌速度、萃取时间等前处理条件。结果表明,以正辛醇为萃取溶剂,0.1 mol·L-1Na OH与300 mg·L-1的Na Cl溶液为供体相,0.1 mol·L-1HCl溶液为接收相,搅拌速度为400 r·min-1,萃取40 min后,3种芳香胺的富集倍数可达48~96倍。该方法对3种痕量芳香胺的线性范围为0.01~0.25 mg·L-1,相关系数（r）不小于0.998 4,检出限为0.3~2.2μg·L-1,相对标准偏差（RSD,n=10）为3.1%~4.0%,用于印染废水中3种芳香胺的分析,回收率为98.0%~102.0%。该方法操作简单,有机溶剂用量少,富集率较高,可用于痕量芳香胺类物质的快速分析。

A new method for the automated determination of three kinds of trace aromatic amines（ otoluidine,3,3＇-dimethylbenzidine, β-naphthyl amine） was developed using on-line hollow fiber liquid-phase microextraction / high performance liquid chromatography. An online detection device was built by connecting the hollow fiber liquid-phase microextraction device and high performance liquid chromatography with sequential injection device. The influences of extraction parameters including extracting solvent,donor phase,acceptor phase,salt effect,stirring rate and extraction time were investigated with this online device. The optimum experimental conditions were as follows： extraction reagent： 1-octanol,donor phase： 0. 1 mol·L- 1Na OH- 300 mg·L- 1Na Cl,acceptor phase： 0. 1mol·L- 1HCl,stirring rate： 400 revolution per minute（ r / min）,extraction time： 40 min. Under the optimum conditions,the qualitative and quantitative analyses of three kinds of trace aromatic amines were preformed by HPLC. The proposed method provided enrichment folds of 48- 96. Good linearities were obtained in the range of 0. 01- 0. 25 mg·L- 1with correlation coefficients not less than0. 998 4. The detection limits（ S / N = 3） were in the range of 0. 3- 2. 2 μg·L- 1,and RSDs（ n = 10）were 3. 1%- 4. 0%. The spiked recoveries of aromatic amines in printing and dyeing wastewater ranged from 98. 0% to 102. 0%. With the advantage of simplicity,rapidness,less consumption of extracting solvent,high enrichment factor,and great precision for detection,this method is effective for fast and accurate analysis of trace aromatic amines.